CN101892495A - Method for producing 4N5 pure indium by electrolyzing high impurity crude indium once - Google Patents
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Abstract
A method for producing 4N5 pure indium by electrolyzing high impurity crude indium once comprises the steps of preparing crude indium anode, preparing starting sheet cathode and conductive bands, preparing electrolyte according to the process requirement and carrying out electrolysis. An electrolytic bath below the crude indium anode is used for electrolysis. The starting sheet cathode is arranged in the electrolytic bath. The distance between different sheets is 25-30mm. The electrolyte is placed into the electrolytic bath and contains 60-80g/l of indium, NaCl with a concentration of 40-60g/l and gelatin with a concentration of 0.2-0.3g/l and has pH value of 2-2.5. The electrolysis temperature is 20-30 DEG C, the current density is 15-25A/m2 and the bath voltage is 0.12-0.18V. The method can realize producing 4N5 pure indium with purity of 99.995% by electrolyzing high impurity crude indium once. In the invention, the starting sheet manufactured by the 4N5 pure indium is used as the cathode, the electrolytic current is stable, precipitation is uniform and the bath voltage is easier to control precisely. Besides, the 4N5 pure indium is produced by electrolyzing once, thus reducing the intermediate links, avoiding production pollution, greatly improving the quality of the pure indium products and lowering the production cost.
Description
Technical field
The invention belongs to field of metallurgy, relate to the production method of the smart indium of a kind of 4N5 of extraction, be applicable to contain from height that (mainly being Gao Xigao lead) once electrolytic production purity reaches the method for purification of the electrorefining indium metal of 99.995% smart indium the assorted thick indium material.
Background technology
Indium is widely used in semi-conductor industry as one of rare metal, also can do senior alloy material, in medical treatment, chemical industry, glass industry, electrical equipment industry extensive use is arranged also, and the metal current indium has become the indispensable important materials of development modern science and technology.In recent years, because country and industry improve the purity of smart indium product to the continuous revision of smart indium product standard gradually.Revise 99.993% by initial 99.99%, revise 99.995% from 99.993% again, its every impurity index all is greatly reduced, and has higher requirement for smart indium production.Original smart indium electrolysis process is difficult to once electrolytic and reaches 99.995% purity, generally adopts twice electrolysis removal of impurities.Along with the zinc smelting system reclaims the abundant of technology, the thick indium quality that comprehensive recovery is produced is also different.Except the thick indium raw material of normal quality, some height contains assorted thick indium, mainly is the thick indium raw material of high lead, high tin impurity, is the difficult point during smart indium is produced.The employed negative electrode of common smart indium electrolysis has two kinds of stainless steel and titanium plates, and stainless steel cathode plate is adopted in 99.993% smart indium electrolysis.After electrolysis finishes, negative electrode and precipitate be washed till neutrality with dilute hydrochloric acid solution and exchanged water after, the glycerine of putting into heating melts, and very easily causes product contamination.Original smart indium electrolysis, in the electrolytic solution since the anode sludge bring into production operation in bring impurity into, and factor such as extraneous contamination in the air, solution suspended substance and impurity particle can appear, cause electrolyte contamination easily, make the electrolytic production downgrade, very difficult once electrolytic reaches 99.995% purity, generally adopts twice electrolysis removal of impurities.The present invention has realized adopting high impurity crude indium once electrolytic to produce the technology of 4N5 essence indium, has improved the scope of application of indium electrolysis tech to raw material, makes smart indium produce electrolysis tech and steps a stage.
Summary of the invention
The purpose of this invention is to provide a kind of high impurity crude indium once electrolytic and produce the method for the smart indium of 4N5, be not only applicable to the thick indium raw material of run-of-the-mill, and be applicable to high impurity crude indium (mainly being high lead, high tin) raw material electrolysis, thereby realize economical with materials consumption, reduce production costs, reduce the production cycle, improve smart indium electrolysis process, the effect that improves production efficiency and product quality.
The technical scheme that adopts is:
High impurity crude indium once electrolytic is produced the method for the smart indium of 4N5, comprises following processing step:
1, the thick indium anode of preparation, thick indium anode is to be raw material with indium master grade 〉=95% high impurity crude indium, make anode except that thallium, vacuum after removing cadmium through conventional chemistry, positive plate is scrubbed with 5% dilute hydrochloric acid, again with exchanged water clean, control does smoothly, wrap under the anode tying of packing into electrolyzer with filter paper for every and treat electrolysis.Thick indium major impurity scope: plumbous≤2.0%, tin≤1.6%, thallium≤1.5%, cadmium≤1.5%, zinc≤1.0%.
2, preparation starting sheet negative electrode and conduction bands.
1. starting sheet preparation: after getting the smart indium of 4N5 and being heated to 160-200 ℃ of fusing slag hitting, on bold and vigorous sheet device, sprinkle into the thick thin slice of 0.5-1mm, be cut into the lengthy motion picture of 200mm * 580-600mm again with the synthetic glass cutter, loading onto current conducting rod at the 460-480mm place makes, the starting sheet negative electrode of making is arranged in the electrolyzer, and the heteropole spacing is 25-30mm;
2. conduction bands preparation: get the smart indium of 4N5 and sprinkle into the 0.8-1.4mm thin slice, be cut into strip, evenly be layered on the both sides at electrolyzer top then, the junction connects tightly with dilute hydrochloric acid, and the conduction bands two ends are connected with the positive and negative electrode terminal of rectifier cabinet (known available product) respectively;
3, according to processing requirement preparation electrolytic solution.Sprinkle to become to approach the indium sheet with the smart indium of 4N5, put into beaker adding sulfuric acid and slowly dissolve, the indium sulfate solution after the dissolving contains indium 60-80g/l.Make liquid pH value reach 2-2.5 with sulfuric acid and exchanged water modulation.Adding NaCl, to make NaCl concentration be 40-60g/1, and adding the gelatin solution that boils again, to make gelatin concentration be 0.2-0.3g/l, after the used for electrolyte quartz pushrod of prepare stirs, measures by setting and to put into electrolyzer;
4, according to electrolysis technology condition energising electrolysis, it is 20-30 ℃ that electrolytic parameter is controlled at electrolysis temperature, and current density is 15-25A/m
2, bath voltage is 0.12-0.18V;
5, in to high impurity crude indium electrolytic process, in order to guarantee that once electrolytic obtains qualified product, adopt electrolyte circulation system, in the circulation of elecrolyte process, Lower tank electrolytic solution is cooled off and purifying treatment, get back in the electrolytic system through falling liquid pump to header tank again.Go out mode on advancing under electrolytic solution adopts in the electrolyzer and circulate, electrolytic solution reaches 100% and filters, cools off and circulation.Per 10 grooves of electrolyzer are one group of circulation, every groove volume 0.06-0.08m
3, size 240mm * 550-600mm * 500mm, per 10 groove flow of electrolyte 0.6-1m
3/ hour, recycle pump regularly 30-40 minute/time;
Electrolysing period 15-20 days, the smart indium of once electrolytic output 4N5.Straight productive rate 〉=50%.With the negative plate washing, ingot casting obtained the smart indium of 4N5 finished product behind the direct fusion after electrolysis finished.
Above-mentioned per-cent is weight percentage.
Above-mentioned current conducting rod is made of stainless steel rod outside volume one deck indium sheet.
In above-mentioned electrolysis process, electrolytic solution can be recycled, and after electrolysis began, electrolyte circulation system was opened, and controls every 30-40 minute automatically and beats liquid, in the working cycle, at Lower tank, the electrolytic solution of inflow is filtered and lowers the temperature.Header tank (inflow) → electrolyzer (overflowing) → Lower tank (filter, cool off) → recycle pump (regularly) → header tank.The recycle system was closed when electrolysis finished, and opened when treating the electrolysis energising again.
Normally carry out for the assurance electrolysis, in time supplemental acid and water are in time checked point of contact and conduction situation, and with preventing poor contact, it is uneven to cause the interpolar groove to press, and quality is separated out in influence.The electrolysis later stage notes preventing situations such as anode and cathode fracture.Cathode breakage is in time repaired with smart indium sheet, otherwise cathode current density is increased and quality is separated out in influence.Anode fracture is in time changed, and prevents that anode from sinking to making the anode sludge enter electrolytic solution and cause product to stain.According to electrolysing period 15-20 days, electrolysis was to the after date outage, and the negative electrode after the fusing obtains 99.995% smart indium product through ingot casting.
The present invention can realize to high impurity crude indium once electrolytic production purity being 99.995% smart indium.
Because the starting sheet that the present invention adopts the smart indium of 4N5 to make is made negative electrode, Faradaic current is stable, separates out evenly, and groove is pressed easier accurate control.In addition,, cut down the number of intermediate links, avoid product contamination, significantly improved smart indium quality product, reduce production costs because once electrolytic makes the smart indium of 4N5.
Embodiment:
Embodiment 1
High impurity crude indium once electrolytic is produced the method for the smart indium of 4N5, comprises following processing step:
1, make anode with thick indium, the thick indium of raw material is mainly impure: Pb≤1.5%, Sn≤1.2%, Zn≤0.5%, Cd≤1.2%, Tl≤1.0%, indium master grade is greater than 95%.Above-mentioned thick indium is carried out vacuum remove cadmium, 800-820 ℃ of vacuum distilling temperature, 12 hours time, vacuum tightness＜0.1Mpa, treatment capacity 50-60kg/ stove.Remove thallium again after removing cadmium earlier, remove 230-250 ℃ of thallium temperature, 50 minutes/time time, number of times 4 times, NH
4Cl: In=75: 1, ZnCl
2: NH
4Cl=3: 1.
To scrub the back except that the thick indium behind the thallium with 5% dilute hydrochloric acid except that cadmium and clean the making anode with exchanged water, anode is contained in the anode after wrapping with filter paper, is arranged in the electrolyzer.
2, make the starting sheet negative electrode with the smart indium of 4N5, the starting sheet negative electrode is: 200 * 580 * 0.5mm, the starting sheet negative electrode is arranged in the electrolyzer, and with anode at a distance of 28mm.
3, electrolytic solution is contained in the electrolyzer by setting quantity, electrolyte PH value is 2.5, and NaCl concentration is 50g/l, gelatin 0.20-0.3g/l, indium 60-80g/l.
4, once electrolytic: groove is pressed 0.12-0.15V, and electrolysis temperature is 20-30 ℃, current density 15-20A/m
2Per 10 groove circulation of elecrolyte flow 0.7-0.8m
3/ hour, electrolysing period 15 days, straight productive rate is 50%.
The outer cooling of electrolytic bath recycles.
By this conditional operation electrolysis, negative electrode indium fusing back sampling is as follows through ICP-MS mass spectrograph checked for impurities: Cu0.0005%, Pb0.0005%, Zn0.0004%, Cd0.0005%, Fe0.0005%, Tl0.0005%, Sn0.0007%, As0.0005%, Al0.0005%, the impurity summation is 0.0046%.
Embodiment 2
High impurity crude indium once electrolytic is produced the method for the smart indium of 4N5, comprises following processing step:
1, make anode with thick indium, the thick indium of raw material mainly contains assorted: Pb≤1.0%, and Sn≤0.8%, Zn≤0.1%, Cd≤0.8%, Tl≤0.8%,, indium master product are greater than 97%.Above-mentioned thick indium is removed cadmium with ordinary method remove thallium, vacuum is removed cadmium: 780-800 ℃ of vacuum distilling temperature, 10 hours time, vacuum tightness＜0.1Mpa, treatment capacity 50-60kg/ stove.Remove thallium after removing cadmium earlier.Chemistry removes 230-250 ℃ of thallium temperature, 50 minutes/time time, number of times 3 times, NH
4Cl: In=75: 1, ZnCl
2: NH
4Cl=3: 1.
To scrub the back except that the thick indium behind the thallium with 5% dilute hydrochloric acid except that cadmium and make anode, be contained in the anode, be arranged in the electrolyzer standby with exchanged water is clean.
2, make the starting sheet negative electrode with the smart indium of 4N5, starting sheet negative electrode specification is 200 * 600 * 1mm, starting sheet is arranged in the electrolyzer, with the anode distance be 30mm.
3, the electrolytic solution (identical with embodiment one) of preparation is put into electrolyzer by setting metering.
4, the once electrolytic groove is pressed 0.15-0.18V, electrolysis temperature 20-30 ℃, pH value 2.0, NaCl concentration 60g/l, gelatin 0.2-0.3g/l, current density 20-25A/m
2, indium 60-80g/l.Every groove circulation of elecrolyte flow 0.6-0.7m
3/ hour, electrolysing period 15-20 days, straight productive rate 〉=55%.
As follows through the general instrument checked for impurities of ICP-MS matter by negative electrode fusing back sampling after this conditional operation electrolysis: Cu0.0003%, Pb0.0005%, Zn0.0004%, Cd0.0005%, Fe0.0005%, Tl0.0005%, Sn0.0005%, As0.0004%, Al0.0005%, the impurity summation is 0.0041%.
Claims (1)
1. high impurity crude indium once electrolytic is produced the method for the smart indium of 4N5, comprises following processing step:
1), the thick indium anode of preparation, thick indium anode is to be raw material with indium master grade 〉=95% high impurity crude indium, make anode except that thallium, vacuum after removing cadmium through conventional chemistry, positive plate is scrubbed with 5% dilute hydrochloric acid, clean, control dried smooth again with exchanged water, wrap the anode of packing into filter paper for every, electrolyzer is treated electrolysis under the tying; Thick indium major impurity scope: plumbous≤2.0%, tin≤1.6%, thallium≤1.5%, cadmium≤1.5%, zinc≤1.0%;
2), preparation starting sheet negative electrode and conduction bands;
1. starting sheet preparation: after getting the smart indium of 4N5 and being heated to 160-200 ℃ of fusing slag hitting, on bold and vigorous sheet device, sprinkle into the thick thin slice of 0.5-1mm, be cut into the lengthy motion picture of 200mm * 580-600mm again with the synthetic glass cutter, loading onto current conducting rod at the 460-480mm place makes, the starting sheet negative electrode of making is arranged in the electrolyzer, and the heteropole spacing is 25-30mm;
2. conduction bands preparation: get the smart indium of 4N5 and sprinkle into the 0.8-1.4mm thin slice, be cut into strip, evenly be layered on the both sides at electrolyzer top then, the junction connects tightly with dilute hydrochloric acid, and the conduction bands two ends are connected with the positive and negative electrode terminal of rectifier cabinet respectively;
3), according to processing requirement preparation electrolytic solution, sprinkle to become to approach the indium sheet with the smart indium of 4N5, put into beaker adding sulfuric acid and slowly dissolve, the indium sulfate solution after the dissolving contains indium 60-80g/l; Make liquid pH value reach 2-2.5 with sulfuric acid and exchanged water modulation; Adding NaCl, to make NaCl concentration be 40-60g/l, and adding the gelatin solution that boils again, to make gelatin concentration be 0.2-0.3g/l, after the used for electrolyte quartz pushrod of prepare stirs, measures by setting and to put into electrolyzer;
4), according to electrolysis technology condition energising electrolysis, it is 20-30 ℃ that electrolytic parameter is controlled at electrolysis temperature, current density is 15-25A/m
2, bath voltage is 0.12-0.18V;
In to high impurity crude indium electrolytic process, obtain qualified product in order to guarantee once electrolytic, adopt electrolyte circulation system, in the circulation of elecrolyte process, Lower tank electrolytic solution is cooled off and purifying treatment, get back in the electrolytic system through falling liquid pump to header tank again; Go out mode on advancing under electrolytic solution adopts in the electrolyzer and circulate, electrolytic solution reaches 100% and filters, cools off and circulation; Per 10 grooves of electrolyzer are one group of circulation, every groove volume 0.06-0.08m
3, size 240mm * 550-600mm * 500mm, per 10 groove flow of electrolyte 0.6-1m
3/ hour, recycle pump regularly 30-40 minute/time;
Electrolysing period 15-20 days, once electrolytic went out the smart indium of 4N5, straight productive rate 〉=50%, and with the negative plate washing, ingot casting obtained the smart indium of 4N5 finished product behind the direct fusion after electrolysis finished;
Above-mentioned per-cent is weight percentage;
Above-mentioned current conducting rod is made of stainless steel rod outside volume one deck indium sheet.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102424990A (en) * | 2011-12-07 | 2012-04-25 | 深圳市危险废物处理站有限公司 | Continuous feeding circulating electrodeposition method |
| CN102492961A (en) * | 2011-12-28 | 2012-06-13 | 株洲科能新材料有限责任公司 | Preparation method of indium electrolyte |
| CN103160855A (en) * | 2011-12-15 | 2013-06-19 | 广东先导稀材股份有限公司 | Preparation method of high-purity indium |
| CN106676579A (en) * | 2017-01-05 | 2017-05-17 | 京东方科技集团股份有限公司 | Method for treating indium tin oxide etching waste liquor |
| CN108262356A (en) * | 2018-01-23 | 2018-07-10 | 内蒙古工业大学 | Indium strip-rolling method |
| CN108823604A (en) * | 2018-08-27 | 2018-11-16 | 云南锡业集团（控股）有限责任公司研发中心 | The method that once electrolytic prepares 5N high purity indium |
| CN110042435A (en) * | 2019-04-06 | 2019-07-23 | 柳州呈奥科技有限公司 | A kind of electrolytic refining process of phosphide material preparation |
| CN110863216A (en) * | 2019-10-28 | 2020-03-06 | 中南大学 | Method for preparing high-purity indium through step cyclone electrodeposition |
| CN112342573A (en) * | 2020-10-20 | 2021-02-09 | 四川大学 | High-efficiency and low-cost sulfate system electrodeposition process for preparing 4N indium |
| CN113668017A (en) * | 2021-08-11 | 2021-11-19 | 广东长信精密设备有限公司 | High-purity indium apparatus for producing |
| CN115044941A (en) * | 2022-06-21 | 2022-09-13 | 成都中建材光电材料有限公司 | Process for preparing high-purity indium by one-step electrolysis of crude indium |
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Cited By (14)
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| CN102424990B (en) * | 2011-12-07 | 2014-07-16 | 深圳市危险废物处理站有限公司 | Continuous feeding circulating electrodeposition method |
| CN102424990A (en) * | 2011-12-07 | 2012-04-25 | 深圳市危险废物处理站有限公司 | Continuous feeding circulating electrodeposition method |
| CN103160855A (en) * | 2011-12-15 | 2013-06-19 | 广东先导稀材股份有限公司 | Preparation method of high-purity indium |
| CN102492961A (en) * | 2011-12-28 | 2012-06-13 | 株洲科能新材料有限责任公司 | Preparation method of indium electrolyte |
| US10202703B2 (en) | 2017-01-05 | 2019-02-12 | Boe Technology Group Co., Ltd. | Method for treating waste liquid from process of etching indium tin oxide |
| CN106676579A (en) * | 2017-01-05 | 2017-05-17 | 京东方科技集团股份有限公司 | Method for treating indium tin oxide etching waste liquor |
| CN108262356A (en) * | 2018-01-23 | 2018-07-10 | 内蒙古工业大学 | Indium strip-rolling method |
| CN108823604A (en) * | 2018-08-27 | 2018-11-16 | 云南锡业集团（控股）有限责任公司研发中心 | The method that once electrolytic prepares 5N high purity indium |
| CN110042435A (en) * | 2019-04-06 | 2019-07-23 | 柳州呈奥科技有限公司 | A kind of electrolytic refining process of phosphide material preparation |
| CN110863216A (en) * | 2019-10-28 | 2020-03-06 | 中南大学 | Method for preparing high-purity indium through step cyclone electrodeposition |
| CN110863216B (en) * | 2019-10-28 | 2020-12-11 | 中南大学 | Method for preparing high-purity indium through step cyclone electrodeposition |
| CN112342573A (en) * | 2020-10-20 | 2021-02-09 | 四川大学 | High-efficiency and low-cost sulfate system electrodeposition process for preparing 4N indium |
| CN113668017A (en) * | 2021-08-11 | 2021-11-19 | 广东长信精密设备有限公司 | High-purity indium apparatus for producing |
| CN115044941A (en) * | 2022-06-21 | 2022-09-13 | 成都中建材光电材料有限公司 | Process for preparing high-purity indium by one-step electrolysis of crude indium |
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